CN107698278A - A kind of method for annealing of ceramic bonnet - Google Patents
A kind of method for annealing of ceramic bonnet Download PDFInfo
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- CN107698278A CN107698278A CN201711053868.8A CN201711053868A CN107698278A CN 107698278 A CN107698278 A CN 107698278A CN 201711053868 A CN201711053868 A CN 201711053868A CN 107698278 A CN107698278 A CN 107698278A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/0072—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5045—Rare-earth oxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04M—TELEPHONIC COMMUNICATION
- H04M1/00—Substation equipment, e.g. for use by subscribers
- H04M1/02—Constructional features of telephone sets
- H04M1/0202—Portable telephone sets, e.g. cordless phones, mobile phones or bar type handsets
- H04M1/026—Details of the structure or mounting of specific components
Abstract
The invention discloses a kind of method for annealing of ceramic bonnet, belong to ceramic bonnet manufacture field, comprise the following steps：Ceramic bonnet is put into annealing furnace, is warming up to 600~800 DEG C of middle temperature area, and be incubated 1~2 hour；After the insulation of middle temperature area, 1000~1200 DEG C of high-temperature area is warming up to, and 3~4 hours are incubated in high-temperature area；After completing soak, 800~900 DEG C are cooled to, time control was at 1~2 hour；Room temperature is naturally cooled to, completion annealing of coming out of the stove.The beneficial effects of the invention are as follows：Using gradient increased temperature and the technique of cooling, by heating up and cooling twice twice, ceramic bonnet is kept for the regular hour in two temperature provinces, ceramic bonnet internal grain is set to grow stage by stage, the interaction force between crystal grain fully discharges, and crystal grain distribution is more uniform, arrangement between crystal grain is more reasonable, so as to effectively reduce caused stress during ceramic bonnet finishing impression, ensure that the ceramic bonnet deflection after annealing within 0.08mm, meets the matching requirements of mobile phone.
Description
Technical field
The present invention relates to ceramic bonnet manufacture field, more particularly to a kind of method for annealing of ceramic bonnet.
Background technology
With the communication 5G epoch, smart mobile phone will abandon existing metal back cover frame completely, and use will not be to signal
Produce shielding ceramic material.Ceramic mobile phone center is as indispensable parts, processing efficiency and product in following cell phone apparatus
Matter is in urgent need to be improved.
Ceramic material can produce certain machining stress after CNC is processed, and this stress can gather in ceramic surface, shadow
The warpage degree of potsherd is rung, serious warpage can produce fragmentation in rear road process, influence the product of whole fabrication cycles
Quality；Stress concentration, centre deformation is also resulted in, ceramic shell is assembled with mobile phone miscellaneous part difficult, finished product is good
Rate is low, not yet occurs the research for more effectively solving ceramic shell buckling deformation at this stage.
Utility model patent if notification number is CN205692182U discloses a kind of zirconia ceramics fingerprint recognition cover plate,
Including fingerprint recognition cover board body, the material of the fingerprint recognition cover plate is zirconia ceramics；The table of the fingerprint recognition cover plate
Face has lappingout superficial layer；The angularity of the fingerprint recognition cover plate is 2 ‰~8 ‰, and thickness is 0.1~1mm, and bending strength is
800~1200Mpa, dielectric constant are 9.4~11.58.This patent does not introduce the specific processing technology of its cover plate.
For another example Publication No. CN106625035A application for a patent for invention discloses a kind of cell phone rear cover 3D zirconium oxides pottery
The processing method of porcelain, its zirconia ceramics used, text in also not over annealing process come reach reduce angularity correlation
Literature record.
The content of the invention
Product warpage is serious, stress concentration to overcome in the prior art, and ceramic shell and the assembling of mobile phone miscellaneous part are tired
Difficulty, the problems such as finished product yield is low, the invention provides a kind of method for annealing of ceramic bonnet, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, annealing furnace is warming up to middle temperature area of the temperature at 600~800 DEG C,
And it is incubated 1~2 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1000~1200 DEG C is warming up to, and in high temperature
Region is incubated 3~4 hours；
Step 3：After completing soak, 800~900 DEG C are cooled to, temperature fall time was controlled at 1~2 hour；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove.
Using gradient increased temperature and the technique of cooling, by heating up and cooling twice twice, ceramic bonnet is two humidity provinces
The regular hour is kept in domain, ceramic bonnet internal grain is grown stage by stage, the interaction force between crystal grain fully discharges,
Crystal grain distribution is more uniform, and the arrangement between crystal grain is more reasonable, so as to be produced during effectively reducing ceramic bonnet finishing impression
Raw stress, ensure the ceramic bonnet deflection after annealing within 0.08mm, to meet mobile phone matching requirements.
Further, the time that middle temperature area is warming up in the step 1 is 3~4 hours.
Further, the time that high-temperature area is warming up in the step 2 is 1~2 hour.
The heating-up time twice of ceramic bonnet is rationally controlled, and coordinates holding stage twice, makes ceramic shell internal oxidation
Thing impurity such as alkaline earth oxide, silica etc. gradually volatilize in higher temperature, efficiently reduce ceramic shell inner oxide
The content of impurity so that the distribution of ceramic bonnet internal grain is more rationally uniform, has more high-quality mechanical property.
Further, annealing furnace is before heating in the step 1, and cover cavity upper side is pressed with one piece of pottery after the ceramics
Porcelain balancing weight, the pressure of the ceramic balancing weight is 5~10N/cm.
When ceramic bonnet is annealed, by applying ceramic bonnet appropriate external pressure, not only can effectively prevent from making pottery
Evagination of the porcelain surface microstructure during rearrangement, and have the function that to eliminate finishing impression machining stress, after reducing ceramics
Cover overall deflection.
Further, in the step 4 in annealing furnace during natural cooling oxygen content between 80~100wt%.
Further, in the step 4 in annealing furnace during natural cooling nitrogen content between 0~15wt%.
Further, in step 1 to annealing furnace in three oxygen content between 50~80wt%, nitrogen content 20~
Between 40wt%, surplus is carbon dioxide.
By controlling furnace annealing atmosphere of annealing, its internal oxygen content is set to be maintained at more than 50wt%, particularly certainly
Right cooling stage, oxygen content are controlled in more than 80wt%, can effectively control grain growth size so that crystal grain is in ceramic shell
Internal distribution is more uniform, and through EMS scanning electron microscopic observations, the size of crystal grain is collocated with each other so that table based on two kinds of diameters
The stomata in face is smaller, more regular and closely knit inside obtained ceramic bonnet.
Further, 760 DEG C are warming up in the step 1 in annealing furnace, and is incubated 1 hour；Heating-up time is 210min,
Heating rate is 3.6 DEG C/min.
Further, 1160 DEG C are warming up in the step 2, and is incubated 3 hours, heating rate is 3.6 DEG C/min.
Further, 900 DEG C are cooled in the step 3, rate of temperature fall is 3.6 DEG C/min.
Further, in the step 4, reach after reaching room temperature inside annealing furnace, open burner hearth, take down ceramic balancing weight,
Ceramic bonnet is taken out, completes annealing.
Further, when cooling is completed in the step 3, impurity is within 1wt% inside ceramic bonnet, the step 4
In when reaching normal temperature in annealing furnace, impurity content is within 0.5wt% inside ceramic bonnet.
Further, during the middle temperature area insulation, RE oxide powder, the rare earth oxygen are uniformly added into annealing furnace
Compound composition is two or more the mixture in Er2O3, NiO, Nd2O3, Gd2O3, Yb2O3 and CeO2, described dilute
The granular size of native oxide powder is 20~50 nanometers.
By adding RE oxide powder into annealing furnace in middle temperature area, rare earth oxide is set to be evenly distributed on ceramics
Enclosure interior, the heat conductivility of ceramic shell is reduced, improve the dimensional stability and visual effect of ceramic shell.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) using gradient increased temperature and the technique of cooling, by heating up and cooling twice twice, ceramic bonnet is in two temperature
The regular hour is kept in region, ceramic bonnet internal grain is grown stage by stage, the interaction force between crystal grain is fully released
Put, crystal grain distribution is more uniform, and the arrangement between crystal grain is more reasonable, so that during effectively reducing ceramic bonnet finishing impression
Caused stress, ensure the ceramic bonnet deflection after annealing within 0.08mm, to meet mobile phone matching requirements；
(2) heating-up time twice of ceramic bonnet is rationally controlled, and coordinates holding stage twice, makes oxygen inside ceramic shell
Compound impurity such as alkaline earth oxide, silica etc. gradually volatilize in higher temperature, efficiently reduce ceramic shell internal oxidition
The content of thing impurity so that the distribution of ceramic bonnet internal grain is more rationally uniform, has more high-quality mechanical property；
(3) when ceramic bonnet is annealed, by applying appropriate external pressure to ceramic bonnet, not only can effectively prevent
Evagination of the ceramic surface crystal grain during rearrangement, and have the function that to eliminate finishing impression machining stress, reduce ceramics
The overall deflection of bonnet；
(4) by controlling furnace annealing atmosphere of annealing, its internal oxygen content is maintained at more than 50wt%, particularly exist
Natural cooling stage, oxygen content are controlled in more than 80wt%, can effectively control grain growth size so that crystal grain is in ceramic case
The distribution in internal portion is more uniform, and through EMS scanning electron microscopic observations, the size of crystal grain is collocated with each other based on two kinds of diameters so that
The stomata on surface is smaller, more regular and closely knit inside obtained ceramic bonnet；
(5) by adding RE oxide powder into annealing furnace in middle temperature area, it is evenly distributed on rare earth oxide
Inside ceramic shell, the heat conductivility of ceramic shell is reduced, improves the dimensional stability and visual effect of ceramic shell.
Embodiment
With reference to embodiments, the present invention will be described in further detail.It is it should be appreciated that described herein specific real
Example is applied only to explain the present invention, is not intended to limit the present invention.
Embodiment one：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1160 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Embodiment two：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 600 DEG C, heating-up time from normal temperature
For 210min, heating rate is 2.8 DEG C/min, and is incubated 2 hours in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1000 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 4 hours in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Embodiment three：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 800 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.8 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1200 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Example IV：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1160 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 800 DEG C are cooled to, cooling rate is controlled in 3.8 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Embodiment five：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 5N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Embodiment six：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 10N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Embodiment seven：
A kind of method for annealing for ceramic bonnet that the present embodiment provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 80wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 10wt%, surplus.
Oxygen content is 50wt% in step 1 to annealing furnace in three, and nitrogen content 40wt%, surplus is carbon dioxide.
Comparative example one：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 500 DEG C, heating-up time from normal temperature
For 210min, heating rate is 2.3 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 900 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 800 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example two：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 500 DEG C, heating-up time from normal temperature
For 210min, heating rate is 2.3 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 950 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example three：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 900 DEG C, heating-up time from normal temperature
For 220min, heating rate is 4.0 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1300 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example four：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1160 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 700 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example five：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1160 DEG C, heating rate 3.6 are warming up to
DEG C/min, and it is incubated 3 hours in high-temperature area；
Step 3：After completing soak, 1000 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example six：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace；Annealing furnace is warming up to the middle warm area that temperature is 760 DEG C from normal temperature
Domain, heating-up time 210min, heating rate are 3.6 DEG C/min, and are incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example seven：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 12N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example eight：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 90wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 5wt%, surplus.
Oxygen content is 40wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Comparative example nine：
A kind of method for annealing for ceramic bonnet that this comparative example provides, comprises the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, cover cavity upper side is pressed with one piece of ceramic balancing weight after ceramics,
The pressure that ceramic balancing weight provides is 7N/cm；Annealing furnace is warming up to the middle temperature area that temperature is 760 DEG C, heating-up time from normal temperature
For 210min, heating rate is 3.6 DEG C/min, and is incubated 1 hour in middle temperature area；
Step 2：After the insulation of middle temperature area, temperature is warming up in 1000~1200 DEG C of high-temperature area, heating rate
For 3.6 DEG C/min, and 3 hours are incubated in high-temperature area；
Step 3：After completing soak, 900 DEG C are cooled to, cooling rate is controlled in 3.6 DEG C/min；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove；Oxygen content is 60wt% during natural cooling, and nitrogen contains
It is carbon dioxide to measure as 15wt%, surplus.
Oxygen content is 60wt% in step 1 to annealing furnace in three, and nitrogen content 30wt%, surplus is carbon dioxide.
Above-mentioned seven groups of embodiments, nine groups of comparative examples and ceramic bonnet sample without annealing are subjected to deformation measurement
Examination, test result are as follows：
According to test result, it can be seen that the ceramic bonnet sample obtained using annealing process in the embodiment of the present invention
Deflection will be significantly less than the ceramic bonnet in comparative example, and the ceramic bonnet after annealing is relative to without annealing
Ceramic bonnet, its deflection obtained very big improvement.
In above-mentioned seven groups of embodiments, when the middle temperature area is incubated, rareearth oxidate powder is uniformly added into annealing furnace
End, the rare earth oxide composition are Er2O3, NiO and Nd2O3 mixture, and the mixed weight percentage of three is 50%：
30%：20%, the granular size of the RE oxide powder is 20~50 nanometers.Its deflection, heat conductivility are examined
Survey, and observe its visual effect, it is found that deflection further reduces, heat conductivility has larger reduction, occurs at night certain
Soft fluorescent effect, and daytime white it is also softer.
The preferred embodiments of the present invention have shown and described in described above, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations, modification and
Environment, and can be changed in the scope of the invention is set forth herein by the technology or knowledge of above-mentioned teaching or association area
It is dynamic., then all should be appended by the present invention and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention
In scope of the claims.
Claims (10)
1. a kind of method for annealing of ceramic bonnet, it is characterised in that comprise the following steps：
Step 1：Ceramic bonnet is put into annealing furnace, annealing furnace is warming up to middle temperature area of the temperature at 600~800 DEG C, and
Middle temperature area is incubated 1~2 hour；
Step 2：After the insulation of middle temperature area, high-temperature area of the temperature at 1000~1200 DEG C is warming up to, and in high-temperature area
Insulation 3~4 hours；
Step 3：After completing soak, 800~900 DEG C are cooled to, temperature fall time was controlled at 1~2 hour；
Step 4：Room temperature is naturally cooled to, completion annealing of coming out of the stove.
2. the method for annealing of a kind of ceramic bonnet according to claim 1, it is characterised in that be warming up in the step 1
The time of middle temperature area is 3~4 hours.
3. the method for annealing of a kind of ceramic bonnet according to claim 1, it is characterised in that be warming up in the step 2
The time of high-temperature area is 1~2 hour.
A kind of 4. method for annealing of ceramic bonnet according to claim 1, it is characterised in that annealing furnace in the step 1
Before heating, cover cavity upper side is pressed with one piece of ceramic balancing weight after the ceramics.
A kind of 5. method for annealing of ceramic bonnet according to claim 1, it is characterised in that annealing furnace in the step 4
Oxygen content is between 80~100wt% during interior natural cooling.
A kind of 6. method for annealing of ceramic bonnet according to claim 5, it is characterised in that annealing furnace in the step 4
Nitrogen content is between 0~15wt% during interior natural cooling.
A kind of 7. method for annealing of ceramic bonnet according to claim 6, it is characterised in that annealing furnace in step 1 to three
Interior oxygen content is between 50~80wt%, and for nitrogen content between 20~40wt%, surplus is carbon dioxide.
A kind of 8. method for annealing of ceramic bonnet according to claim 1, it is characterised in that annealing furnace in the step 1
760 DEG C are inside warming up to, and is incubated 1 hour；Heating-up time is 210min, and heating rate is 3.6 DEG C/min.
9. the method for annealing of a kind of ceramic bonnet according to claim 8, it is characterised in that be warming up in the step 2
1160 DEG C, and 3 hours are incubated, heating rate is 3.6 DEG C/min.
10. the method for annealing of a kind of ceramic bonnet according to claim 9, it is characterised in that cool in the step 3
To 900 DEG C, rate of temperature fall is 3.6 DEG C/min.
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